HRID501967
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
To a solution of (±)-2-hydroxy-3-(7-methyl-2-((2-(trimethylsilyl)ethoxy)methyl)-2H-indazol-5-yl)propanoic acid (100 mg, 0.29 mmol), 4-piperidinopiperidine (96.0 mg, 2.0 equiv), and diisopropylethylamine (0.10 mL, 0.57 mmol) in dichloromethane (3.6 mL) at 0° C. was added PyBOP® (156 mg, 0.30 mmol) in two portions. The reaction was stirred at 0° C. for 15 minutes and at room temperature overnight. The reaction was diluted with ethyl acetate, washed with water (2×), then brine, dried over magnesium sulfate, and concentrated. Column chromatography (4% to 10% methanol/dichloromethane) gave 130 mg (91%) as an oil. Mass spec.: 501.36 (MH)+.
WORKUP
后处理
- washwashed with water (2×)
- dry with materialbrine, dried over magnesium sulfate
- concentrationconcentrated
- customColumn chromatography (4% to 10% methanol/dichloromethane) gave 130 mg (91%) as an oil